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GB/T 13747.13-2017: Methods for chemical analysis of zirconium and zirconium alloys -- Part 13: Determination of lead content -- Polarography
Status: Valid GB/T 13747.13: Evolution and historical versions
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| GB/T 13747.13-2017 | English | 119 |
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Methods for chemical analysis of zirconium and zirconium alloys -- Part 13: Determination of lead content -- Polarography
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GB/T 13747.13-2017
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| GB/T 13747.13-1992 | English | 159 |
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Zirconium and zirconium alloys. Determination of lead content. Oscillopolarographic method
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GB/T 13747.13-1992
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Basic data | Standard ID | GB/T 13747.13-2017 (GB/T13747.13-2017) | | Description (Translated English) | Methods for chemical analysis of zirconium and zirconium alloys -- Part 13: Determination of lead content -- Polarography | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | H63 | | Classification of International Standard | 77.120.99 | | Word Count Estimation | 6,690 | | Date of Issue | 2017-09-29 | | Date of Implementation | 2018-04-01 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | GB/T 13747.13-2017: Methods for chemical analysis of zirconium and zirconium alloys -- Part 13: Determination of lead content -- Polarography
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Methods for chemical analysis of zirconium and zirconium alloys - Part 13. Determination of lead content - Polarography
ICS 77.120.99
H63
National Standards of People's Republic of China
Replacing GB/T 13747.13-1992
Methods for chemical analysis of zirconium and zirconium alloys
Part 13. Determination of lead content
Polarographic method
Methods for chemical analysis of zirconiumiumandzirconiumaloys-
Part 13.Determinationofleadcontent-
Polarography
2017-09-29 Posted
2018-04-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
GB/T 13747 "zirconium and zirconium alloy chemical analysis method" is divided into 27 parts.
--- Part 1. Determination of tin content potassium iodate titration and phenylfluorone - polyethylene glycol octyl phenyl ether spectrophotometry;
--- Part 2. Determination of iron content 1,10-phenanthroline spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 3. Determination of nickel content dimethylglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 4. Determination of chromium content Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 5. Determination of aluminum content chrome azure S-tetradecyl pyridine chloride spectrophotometry;
--- Part 6. Determination of copper content 2,9-dimethyl-1,10-phenanthroline spectrophotometry;
--- Part 7. Determination of manganese content potassium periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 8. Determination of cobalt content Nitroso R salt spectrophotometry;
--- Part 9. Determination of magnesium content by flame atomic absorption spectrometry;
--- Part 10. Determination of tungsten content thiocyanate spectrophotometry;
--- Part 11. Determination of molybdenum content thiocyanate spectrophotometry;
--- Part 12. Determination of silicon content Molybdenum blue spectrophotometry;
--- Part 13. Determination of lead content polarographic method;
--- Part 14. Determination of uranium volume Polarographic method;
--- Part 15. Determination of boron content curcumin spectrophotometry;
--- Part 16. Determination of chlorine content of silver chloride turbidity and ion selective electrode method;
--- Part 17. Determination of cadmium content Polarographic method;
--- Part 18. Determination of vanadium content; Benzoylphenylhydroxylamine spectrophotometry;
--- Part 19. Determination of titanium content diantipyryl methane spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 20. Determination of hafnium content Inductively coupled plasma atomic emission spectrometry;
--- Part 21. Determination of hydrogen content inert gas melting infrared absorption method/thermal conductivity method;
Part 22 - Determination of oxygen and nitrogen content - Inert gas fusion infrared absorption method/Thermal conductivity method;
--- Part 23. Determination of nitrogen content Distillation separation - Nessler reagent spectrophotometry;
--- Part 24. Determination of carbon content High-frequency combustion infrared absorption method;
--- Part 25. Determination of niobium content 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry;
--- Part 26. Determination of alloying and impurity elements; Inductively coupled plasma atomic emission spectrometry;
--- Part 27. Determination of trace impurity elements Inductively coupled plasma mass spectrometry.
This section GB/T 13747 Part 13.
This section drafted in accordance with GB/T 1.1-2009 given rules.
This Part replaces GB/T 13747.13-1992 "zirconium and zirconium alloy chemical analysis methods oscillopolarographic determination of lead content." This section and
GB/T 13747.13-1992 compared to editorial changes in addition to the main technical changes are as follows.
--- Removed the "reference standard" (Chapter.1992 of Chapter 2);
--- Increase the sample terms (see Chapter 5);
--- Increase the precision clause (see Chapter 8, Chapter 8 of the.1992 edition);
--- Added test report terms (see Chapter 9).
This part is proposed by China Nonferrous Metal Industry Association.
This part of the National Non-ferrous Metal Standardization Technical Committee (SAC/TC243) centralized.
This part of the drafting unit. Western Metal Materials Co., Ltd., Exit Inspection and Quarantine of Hunan Province, Northwest Nonferrous Metal Research Institute, Guangdong
Provincial Industrial Analysis and Testing Center, Beijing Mining and Metallurgical Research Institute.
The main drafters of this section. Liu Hou Yong, Yang Junhong, Wang Xiaofei, Zhai Tongde, Yang Wanbiao, Lu small Park, Wang Jinlei, Yang Ping, Xiong Xiaoyan,
Chuang Ai Chun, Li Min, Liu Wei.
This part replaces the standards previously issued as.
--- GB/T 13747.13-1992.
Methods for chemical analysis of zirconium and zirconium alloys
Part 13. Determination of lead content
Polarographic method
1 Scope
GB/T 13747 provisions of this part of zirconium and zirconium alloy determination of the amount of lead.
This section applies to sponge zirconium, zirconium and zirconium alloy determination of the amount of lead. Measurement range. 0.0005% ~ 0.030%.
2 method summary
The sample is dissolved in hydrofluoric acid, the zirconium is masked with ammonium citrate, and the mixture is extracted with dithizone-chloroform in an ammonia medium having a pH of 9 to 10
Lead, measured by linear sweep polarography in dilute hydrochloric acid at the bottom.
3 Reagents and materials
Unless otherwise noted, only reagents identified as superior pure and laboratory grade II water were used in the analysis.
3.1 Hydrofluoric acid (p = 1.15 g/mL).
3.2 Nitric acid (p = 1.42 g/mL).
3.3 Perchloric acid (ρ = 1.68g/mL).
3.4 Ammonia (ρ = 0.9g/mL) Liquid ammonia is absorbed and purified by distilled water.
3.5 Hydrochloric acid [c (HCl) = 0.5 mol/L].
3.6 triammonium citrate solution (300g/L). Weigh 150g of triammonium citrate dissolved in about 300mL water was added 100mL saturated boric acid
Liquid, diluted with water to 500mL volume, mix.
3.7 Dithizone - chloroform extract (0.5g/L). Weigh 2.5g dithizone dissolved in about 400mL of chloroform, into 1000mL points
Liquid funnel. Add.200mL ammonia (1 9), shake 3min. After stratification, the organic phase was placed in another separatory funnel and the aqueous phase was added
500mL beaker retained. The organic phase was added.200mL ammonia (1 9) extracted once, the organic phase was discarded. The combined aqueous phase, with degreasing
Cotton filter to remove insoluble material. Hydrochloric acid was added dropwise to acidify the aqueous phase, and the dithizone precipitate was completely transferred to a separatory funnel. A total of 500mL three times in three
The chloroform was extracted by shaking to dissolve the dithizone in the organic phase. The combined organic phases were washed once with 500 mL of water and the organic phase was in a brown bottle
Save sealed. This organic phase 1L containing 5g dithizone, when used to dilute the preparation of chloroform.
3.8 Ammonium citrate - aqueous ammonia washing solution Each 100mL solution contains 3g ammonium citrate, 1mL ammonia (3.4).
3.9 Lead standard solution A. Weigh 0.1000g metal lead (wPb ≥ 99.9%) was dissolved in 30mL of nitric acid (1 2), heated to remove nitrogen oxygen
Chemical, cooling. Into a 1000mL volumetric flask, diluted with water to the mark, mix well. 1 mL of this solution contains 100 μg lead.
3.10 Lead standard solution B. Pipette 50.00mL lead standard solution A (3.9) in 500mL volumetric flask, diluted with water to the mark, and mix.
1 mL of this solution contains 10 μg of lead.
3.11 nitrogen (volume fraction ≥ 99.99%).
4 instruments
Polarographic analyzer. Droplet mercury electrode, mercury pool anode or three-electrode system.
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